鸦胆子中苦木内酯类化合物的制备分离和化学表征

Isolation and Identification of Quassinoids from Brucea Javanica (L.) Merr

研究制备型高效液相色谱分离纯化鸦胆子中3个苦木内酯的方法。制备色谱的参数为:色谱柱为C18柱(50 mm×200 mm,5μm),流动相为甲醇-水(体积比为40∶60),流速100 mL/min,二级管阵列检测器检测波长为270 nm,进样体积为2 mL。在30 min的运行时间内,鸦胆苦素D,鸦胆苦醇与鸦胆因H与干扰成分得到很好的分离,经HPLC和熔点测定等方法检测纯度均达到98%以上,化学结构由核磁共振氢谱和碳谱进一步确认。此方法具有快速高效、分离组分纯度高的特点,可用于制备鸦胆苦素D、鸦胆苦醇及鸦胆因H。

The objective of this study is to develop a preparative high performance liquid chromatography （HPLC） method for the isolation and purification of three quassinoids from Brucea javanica （ L. ） Merr. The optimum operation param eters were selected as follows：a Cis column （50 mm x 200 mm,5 Ixm） with methanol-water （40： 60,v/v） as the mo bile phase at a flow rate of 100 mL/min, the detection wavelength of 270 nm, and the injection volume of 2 mL. Bruceine D, brusatol and brueeine H can be obtained in a 30 min, and the purities of the products were detected by melting point and HPLC method. The results displayed that the purities of products were above 98%. The effective and rapid method was successfully applied for isolating bruceine D, brusatol and bruceine H from Brucea javanica （L.） MelT.